CN108670953B - Dihydromyricetin water-soluble nano suspending agent and preparation method and application thereof - Google Patents
Dihydromyricetin water-soluble nano suspending agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of preparations, and particularly relates to a dihydromyricetin water-soluble nano suspending agent, and a preparation method and application thereof. The invention provides a preparation method of a dihydromyricetin water-soluble nano suspending agent, which comprises the following steps: a) mixing oil phase dissolved with dihydromyricetin and water solution dissolved with emulsifier uniformly, emulsifying, and homogenizing under high pressure to obtain O/W type nanometer emulsion; b) drying the O/W type nano emulsion to obtain dihydromyricetin nano particles; c) and mixing the dihydromyricetin nano particles with water, and dispersing to obtain the dihydromyricetin water-soluble nano suspending agent. According to the preparation method, O/W type nano emulsion is obtained through high-pressure homogenization, then drying is carried out to obtain dihydromyricetin nano particles, and the dihydromyricetin nano particles are mixed with water to prepare the dihydromyricetin water-soluble nano suspending agent, so that the solubility of the dihydromyricetin in water is improved, and the application of the dihydromyricetin in the fields of food and medical industries is expanded.
Description
Technical Field
The invention belongs to the technical field of preparations, and particularly relates to a dihydromyricetin water-soluble nano suspending agent, and a preparation method and application thereof.
Background
Dihydromyricetin, also known as ampelopsin, fujianzhain, ampelopsin, and the like, belongs to flavanonols compounds and is a main active ingredient of Ampelopsis grossedentata of Ampelopsis of Vitaceae. Dihydromyricetin has multiple biological activities and good safety, but has poor stability and low solubility in water. The solubility of dihydromyricetin in water at 25 deg.C is 0.2 mg/mL. When the dihydromyricetin is taken into a human body, the solubility of the fat-soluble dihydromyricetin in water which is a main component in the human body is poor, so that the bioavailability of the dihydromyricetin is low, and the dihydromyricetin is accompanied by toxic and side effects, thereby limiting the application of the dihydromyricetin in medicines, foods and cosmetics.
In order to improve the water solubility of the dihydromyricetin, a large number of innovative researches are carried out by scholars at home and abroad, and the method for improving the water solubility mainly comprises the step of preparing the dihydromyricetin into preparations such as liposome, microemulsion, microcapsule, inclusion compound, nano micelle and the like so as to achieve the purposes of improving the solubility of the dihydromyricetin and improving the stability and bioavailability of the dihydromyricetin. However, the preparation process of liposome, microemulsion, microcapsule, etc. is complicated and is difficult to control effectively.
Nanotechnology has developed rapidly in recent years, and nanosuspensions have become an important development direction in the field of pharmaceutical preparations. However, the existing nano suspending agent has some defects, most of the nano suspending agents use organic solvents which can pollute the environment during preparation, the preparation process has high energy consumption, high cost and great difficulty, industrial production cannot be realized, and difficulty is brought to application.
Disclosure of Invention
In view of the above, the invention provides a dihydromyricetin water-soluble nano suspending agent, and a preparation method and an application thereof, and aims to solve the problems that dihydromyricetin is poor in water solubility, an organic solvent which pollutes the environment is required to be used in the preparation of the nano suspending agent, the energy consumption in the preparation process is high, and the like.
The specific technical scheme of the invention is as follows:
a preparation method of a dihydromyricetin water-soluble nano suspending agent comprises the following steps:
a) mixing oil phase dissolved with dihydromyricetin and water solution dissolved with emulsifier uniformly, emulsifying, and homogenizing under high pressure to obtain O/W type nanometer emulsion;
b) drying the O/W type nano emulsion to obtain dihydromyricetin nano particles;
c) and mixing the dihydromyricetin nano particles with water, and dispersing to obtain the dihydromyricetin water-soluble nano suspending agent.
Preferably, the particle size of dihydromyricetin in the O/W type nano emulsion in the step a) is 50 nm-100 nm.
Preferably, the pressure of the high-pressure homogenization in the step a) is 900bar to 1000 bar;
the high-pressure homogenizing time is 5-10 min.
Preferably, the stirring speed of the emulsification in the step a) is 8000-15000 rpm, and the emulsification time is 5-10 min.
Preferably, the volume ratio of the oil phase to the aqueous solution in the step a) is 1-3: 7 to 9.
Preferably, the drying in step b) is freeze-drying;
the temperature of the freeze drying is-60 ℃ to-40 ℃;
the freeze drying time is 24-48 h.
Preferably, said dispersing in step c) comprises ultrasonic dispersing;
the power of the ultrasonic dispersion is 200W-400W.
Preferably, the mass ratio of the dihydromyricetin nanoparticles to the water in the step c) is 10-15: 100.
the invention also provides a dihydromyricetin water-soluble nano suspending agent prepared by the preparation method of the technical scheme.
The invention also provides application of the water-soluble nano suspending agent in preparation of medicines and/or foods.
In summary, the invention provides a preparation method of a dihydromyricetin water-soluble nano suspending agent, which comprises the following steps: a) mixing oil phase dissolved with dihydromyricetin and water solution dissolved with emulsifier uniformly, emulsifying, and homogenizing under high pressure to obtain O/W type nanometer emulsion; b) drying the O/W type nano emulsion to obtain dihydromyricetin nano particles; c) and mixing the dihydromyricetin nano particles with water, and dispersing to obtain the dihydromyricetin water-soluble nano suspending agent. The preparation method of the invention obtains O/W type nano emulsion by mechanical forces of high speed, high pressure and high frequency impact, collision, shearing, grinding, vibration, dispersion and the like generated by high pressure homogenization on the premise of not changing the chemical structure of the dihydromyricetin, and the dihydromyricetin nano particles obtained by drying the O/W type nano emulsion are mixed with water to ensure that the dihydromyricetin can be completely dissolved and uniformly dispersed in the water to prepare the dihydromyricetin water-soluble nano suspending agent, thereby solving the problem of low solubility of the dihydromyricetin in the water and expanding the application of the dihydromyricetin in the fields of food and medical industry. In addition, the preparation method does not need to use an organic solvent which causes environmental pollution, is green and environment-friendly, is simple to operate, has low energy consumption and low cost, and is easy to realize industrial production.
Detailed Description
The invention provides a dihydromyricetin water-soluble nano suspending agent, and a preparation method and application thereof, and aims to solve the problems that dihydromyricetin is poor in water solubility, an organic solvent is required to be used during preparation of the nano suspending agent, the environment is polluted, the energy consumption in the preparation process is high, and the like.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of a dihydromyricetin water-soluble nano suspending agent comprises the following steps:
a) mixing oil phase dissolved with dihydromyricetin and water solution dissolved with emulsifier uniformly, emulsifying, and homogenizing under high pressure to obtain O/W type nanometer emulsion;
b) drying the O/W type nano emulsion to obtain dihydromyricetin nano particles;
c) and mixing the dihydromyricetin nano particles with water, and dispersing to obtain the dihydromyricetin water-soluble nano suspending agent.
The preparation method of the invention obtains O/W type nano emulsion by mechanical forces of high speed, high pressure and high frequency impact, collision, shearing, grinding, vibration, dispersion and the like generated by high pressure homogenization on the premise of not changing the chemical structure of the dihydromyricetin, and the dihydromyricetin nano particles obtained by drying the O/W type nano emulsion are mixed with water to ensure that the dihydromyricetin can be completely dissolved and uniformly dispersed in the water to prepare the dihydromyricetin water-soluble nano suspending agent, thereby solving the problems of low solubility and poor stability of the dihydromyricetin in the water, expanding the application of the dihydromyricetin in the fields of food and medicine industry and improving the using effect of the dihydromyricetin. In addition, the preparation method does not need to use an organic solvent which causes environmental pollution, is green and environment-friendly, is simple to operate, has low energy consumption and low cost, and is easy to realize industrial production.
In the invention, the grain diameter of dihydromyricetin in the O/W type nano emulsion in the step a) is 50 nm-100 nm.
The concentration of the dihydromyricetin in the oil phase in which the dihydromyricetin is dissolved in the step a) is 3 mg/ml-10 mg/ml.
In the present invention, the oil phase comprises one or more of Capmul MCM C8, Capmul MCM C10, Capmul MCM, CAPTEX355, MAISINE35-1 and soybean oil. Capmul MCM C8 is caprylic acid C8 monoglyceride or diester, Capmul MCM C10 is coconut oil C10 monoglyceride or diester, Capmul MCM is a mixture of medium chain monoglyceride and diester, CAPTEX355 is caprylic/capric triglyceride, and MAISINE35-1 is monoglyceride.
The water solution dissolved with the emulsifier in the step a) is a water phase, the emulsifier in the water phase comprises one or more of span-80, span-60, span-20, tween-60, tween-80, propylene glycol alginate, molecular distillation monoglyceride and octenyl sodium starch succinate, and the mass ratio of the emulsifier to the water refers to the product specification of span-80, span-60, span-20, tween-60, tween-80, propylene glycol alginate, molecular distillation monoglyceride and/or octenyl sodium starch succinate.
The oil phase used in the preparation method belongs to an organic solvent which does not pollute the environment, the oil phase and the emulsifier used in the preparation method are both food grade, and the prepared dihydromyricetin water-soluble nano suspending agent can be used for preparing medicines and/or foods.
In the invention, the pressure of the high-pressure homogenization in the step a) is 900 bar-1000 bar.
The time of high-pressure homogenization is 5min to 10 min.
The times of high-pressure homogenization are 8-12 times.
The oil phase dissolved with dihydromyricetin and the emulsion of the water solution dissolved with the emulsifier are subjected to high-pressure homogenization with the pressure of 900 bar-1000 bar and the times of 8-12 times, and the O/W type nano emulsion is obtained by mechanical forces of high-speed, high-pressure and high-frequency impact, collision, shearing, grinding, vibration, dispersion and the like generated by the high-pressure homogenization on the premise of not changing the chemical structure of the dihydromyricetin.
In the invention, the step a) of uniformly mixing comprises the following steps:
slowly pouring the oil phase dissolved with the dihydromyricetin into the water solution dissolved with the emulsifier under the stirring of 100 rpm-200 rpm, and stirring and mixing for 10 min-30 min at the speed of 800 rpm-1500 rpm.
The stirring speed of emulsification in the step a) is 8000-15000 rpm, and the emulsification time is 5-10 min.
In the invention, the volume ratio of the oil phase to the aqueous solution in the step a) is 1-3: 7 to 9.
The drying in the step b) is freeze drying;
the temperature of freeze drying is-60 ℃ to-40 ℃;
the freeze drying time is 24-48 h.
Under the condition of freeze drying, according to the ice crystal sublimation principle, the O/W type nano emulsion is converted into freeze-dried emulsion in a high-vacuum environment, and aggregation, fusion and leakage of an encapsulated substance can be prevented during storage.
In the invention, the dispersion in the step c) is specifically carried out under the condition of water bath at the temperature of 20-30 ℃. The dispersion time is 20-40 min.
The dispersing in step c) comprises ultrasonic dispersing;
the power of ultrasonic dispersion is 200W-400W;
the frequency of ultrasonic dispersion was 20 Hz.
During the ultrasonic dispersion in the step c), stirring is also carried out;
the stirring speed of the stirring is 100 rpm-500 rpm;
in the step c), the mass ratio of the dihydromyricetin nanoparticles to water is 10-15: 100.
the preparation method of the invention prepares the nano emulsion by mechanical force on the premise of not changing the chemical structure of the dihydromyricetin, and then dries to obtain the dihydromyricetin nano particle, wherein the particle size of the dihydromyricetin nano particle is 50 nm-100 nm, and the dihydromyricetin nano particle can be completely dissolved and uniformly dispersed in aqueous solution to form the dihydromyricetin water-soluble nano suspending agent, thereby increasing the hydrophilicity of the dihydromyricetin, having good dispersibility in the dihydromyricetin, solving the problem of solubility of the dihydromyricetin in the aqueous solution, keeping the effective components of the dihydromyricetin well, enlarging the application range and improving the use effect. In addition, the preparation method is simple to operate, has no pollution, can realize the controllability of the nanometer particle size of the dihydromyricetin, has good repeatability, and ensures that the quality of the dihydromyricetin water-soluble nanometer suspending agent is easy to control.
The invention also provides the dihydromyricetin water-soluble nano suspending agent prepared by the preparation method of the technical scheme.
The oil phase and the emulsifier used in the preparation method are both food grade, and the invention also provides the application of the water-soluble nano suspending agent in the technical scheme in the preparation of medicines and/or foods.
For a further understanding of the invention, reference will now be made in detail to the following examples.
Example 1
(1) Preparing an oil phase with the content of dihydromyricetin of 5% (W/V) by using Capmul MCM C8 as an organic solvent; selecting Tween-20 as emulsifier, preparing 0.5% (W/V) aqueous solution of emulsifier, and making into water phase. Slowly pouring the oil phase into the water phase under stirring at the rotating speed of 100rpm, wherein the volume ratio of the oil phase to the water phase is 1: and 9, continuing to stir at the rotating speed of 800rpm for 30min, and uniformly mixing. Stirring and emulsifying the obtained mixed solution for 10min at the rotation speed of 8000rpm, and then carrying out high-pressure homogenization for 12 times under the pressure of 800bar, wherein the high-pressure homogenization time is 5min each time, so as to obtain O/W type nano emulsion, wherein the particle size of dihydromyricetin in the O/W type nano emulsion is 50 nm-100 nm.
(2) Freeze-drying the O/W type nano emulsion at-40 deg.C for 48h to obtain dihydromyricetin nanoparticles;
(3) mixing dihydromyricetin nano particles and water according to a mass ratio of 1: 10, and stirring the mixture for 40min at 100rpm by using 200W ultrasonic oscillation under the condition of water bath at the temperature of 20 ℃ to obtain the fully dispersed dihydromyricetin water-soluble nano suspending agent. The detection result shows that the solubility of the dihydromyricetin in the dihydromyricetin water solution nanometer suspending agent is 3.12mg/mL, the average particle size of the dihydromyricetin is 50nm, and the polydispersity index of the dihydromyricetin is 0.083.
Example 2
(1) Using CAPTEX355 as organic solvent, and preparing oil phase with dihydromyricetin content of 8% (W/V); span-80 is selected as an emulsifier, and an aqueous solution with the emulsifier concentration of 0.5% (W/V) is prepared to prepare a water phase. Slowly pouring the oil phase into the water phase under the stirring of the rotating speed of 150rpm, wherein the volume ratio of the oil phase to the water phase is 2: and 8, continuing to stir at the rotation speed of 900rpm for 20min, and uniformly mixing. Stirring and emulsifying the obtained mixed solution for 8min at the rotation speed of 10000rpm, and then carrying out high-pressure homogenization for 10 times under the pressure of 900bar, wherein the high-pressure homogenization time for each time is 8min, so as to obtain O/W type nano emulsion, wherein the particle size of dihydromyricetin in the O/W type nano emulsion is 50 nm-100 nm.
(2) Freeze-drying the O/W type nano emulsion at-50 deg.C for 36h to obtain dihydromyricetin nanoparticles;
(3) mixing dihydromyricetin nano particles with water according to the mass ratio of 3: 25, and stirring the mixture for 30min at 200rpm under the water bath condition of 25 ℃ by using 300W ultrasonic oscillation to obtain the fully dispersed dihydromyricetin water-soluble nano suspending agent. The detection result shows that the solubility of the dihydromyricetin in the dihydromyricetin water solution nanometer suspending agent is 6.86mg/mL, the average particle size of the dihydromyricetin is 80nm, and the polydispersity index of the dihydromyricetin is 0.121.
Example 3
(1) Preparing an oil phase with the content of dihydromyricetin of 10% (W/V) by taking soybean oil as an organic solvent; selecting sodium starch octenyl succinate as emulsifier, preparing 0.5% (W/V) water solution of emulsifier, and making into water phase. Slowly pouring the oil phase into the water phase under the stirring of the rotating speed of 200rpm, wherein the volume ratio of the oil phase to the water phase is 3: and 7, continuing to stir at the rotating speed of 1000rpm for 10min, and uniformly mixing. Stirring and emulsifying the obtained mixed solution for 5min at the rotation speed of 15000rpm, and then carrying out high-pressure homogenization for 8 times under the pressure of 1000bar, wherein the high-pressure homogenization time for each time is 10min, so as to obtain O/W type nano emulsion, wherein the particle size of dihydromyricetin in the O/W type nano emulsion is 50 nm-100 nm.
(2) Freeze-drying the O/W type nano emulsion at-60 deg.C for 24h to obtain dihydromyricetin nanoparticles;
(3) mixing dihydromyricetin nano particles with water according to the mass ratio of 3: 20, and stirring the mixture for 20min at the water bath condition of 30 ℃ by using 300W ultrasonic oscillation and 500rpm to obtain the fully dispersed dihydromyricetin water-soluble nano suspending agent. The detection result shows that the solubility of the dihydromyricetin in the dihydromyricetin water solution nanometer suspending agent is 8.35mg/mL, the average particle size of the dihydromyricetin is 100nm, and the polydispersity index of the dihydromyricetin is 0.173.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of a dihydromyricetin water-soluble nano suspending agent is characterized by comprising the following steps:
a) mixing oil phase dissolved with dihydromyricetin and water solution dissolved with emulsifier uniformly, emulsifying, and homogenizing under high pressure to obtain O/W type nanometer emulsion;
b) drying the O/W type nano emulsion to obtain dihydromyricetin nano particles;
c) mixing the dihydromyricetin nano particles with water, and dispersing to obtain a dihydromyricetin water-soluble nano suspending agent;
the volume ratio of the oil phase to the aqueous solution is 1-3: 7-9;
the oil phase is selected from one or more of Capmul MCM C8, Capmul MCM C10, Capmul MCM, CAPTEX355, MAISINE35-1 and soybean oil;
the emulsifier is one or more selected from span-80, span-60, span-20, tween-60, tween-80, propylene glycol alginate, molecular distillation monoglyceride and octenyl succinic acid starch ester sodium;
the particle size of the dihydromyricetin nano-particles is 50 nm-100 nm;
the pressure intensity of the high-pressure homogenization is 900 bar-1000 bar;
the high-pressure homogenizing time is 5-10 min.
2. The method according to claim 1, wherein the stirring speed of the emulsification in the step a) is 8000rpm to 15000rpm, and the time of the emulsification is 5min to 10 min.
3. The method of claim 1, wherein the drying in step b) is freeze-drying;
the temperature of the freeze drying is-60 ℃ to-40 ℃;
the freeze drying time is 24-48 h.
4. The method of claim 1, wherein the dispersing in step c) comprises ultrasonic dispersing;
the power of the ultrasonic dispersion is 200W-400W.
5. The preparation method according to claim 1, wherein the mass ratio of the dihydromyricetin nanoparticles to the water in the step c) is 10-15: 100.
6. the dihydromyricetin water-soluble nano suspending agent prepared by the preparation method of any one of claim 1 to claim 5.
7. Use of the water-soluble nanosuspension of claim 6 in the preparation of a medicament and/or a food product.
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| CN109717351B (en) * | 2018-12-28 | 2022-07-05 | 广东工业大学 | Ampelopsin and metal ion composite emulsion bacteriostatic agent as well as preparation method and application thereof |
| CN109924491A (en) * | 2019-04-01 | 2019-06-25 | 东南大学 | A kind of dihydromyricetin solid-state self-emulsifying material and its preparation method and application |
| CN114404369B (en) * | 2022-03-08 | 2023-01-03 | 陕西科技大学 | Dihydromyricetin nanocrystal and preparation method and application thereof |
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